CN113354320A - Nano silicon-titanium powder material and preparation method thereof - Google Patents
Nano silicon-titanium powder material and preparation method thereof Download PDFInfo
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- CN113354320A CN113354320A CN202110650940.5A CN202110650940A CN113354320A CN 113354320 A CN113354320 A CN 113354320A CN 202110650940 A CN202110650940 A CN 202110650940A CN 113354320 A CN113354320 A CN 113354320A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
Abstract
A nanometer silicon-titanium powder material and a preparation method thereof comprise the following steps: s1, uniformly mixing raw materials, and feeding the raw materials into a plasma electric furnace in a protective gas atmosphere; introducing hydrogen-containing protective gas into the furnace, heating, and carrying out high-temperature melt mixing; s2, enabling the molten and mixed liquid flow to flow into a graphite cyclone separator, separating liquid silicon-containing raw materials, sending the liquid silicon-containing raw materials into a laser generator, directly radiating the molten raw materials by generated laser, and enabling the silicon-containing raw materials to quickly reach a boiling point and evaporate and gasify the silicon-containing raw materials into silicon vapor by utilizing a laser radiation effect; silicon vapor is sucked into a cooler and is rapidly cooled to 1120-1240 ℃, and is naturally cooled for subsequent treatment after being mixed with other melt mixtures. The composite silicon powder obtained by adopting the nano silicon-titanium powder material and the preparation method thereof has the bulk density of 0.9-1.5 g/cm3, and has the characteristics of large particle size span, excellent micro-gradation, good dispersion performance, obvious reduction of water requirement ratio when being doped into concrete, effective reduction of concrete shrinkage rate and the like.
Description
Technical Field
The invention belongs to the technical field of materials, relates to a silicon powder improvement technology, and particularly relates to a nano silicon-titanium powder material and a preparation method thereof.
Background
The combination of the nano material modified concrete as a traditional material and a new material technology is a new direction for the development of the concrete industry in recent years. The nano material modified concrete not only improves the strength and durability of the original cement-based concrete, but also has some special functions of the nano material, and researches show that the early strength can be improved by 30-40% only by adding 1% of the nano material by using the Portland cement.
At present, factors for restricting the large-scale use of the nano material are mainly complex raw material processing technology, concentrated release of cement hydration heat and agglomeration generated by high surface energy of the nano material, and in addition, the price is also a non-negligible factor. At present, research and engineering application aiming at the nano material modified high-performance concrete mainly focus on three directions: firstly, the preparation and application technology of the high-crystallinity nano material, and secondly, the influence and mechanism of the nano material on the performance of the silicate cement slurry; thirdly, the mechanical property and the durability of the internally doped nano material to the high-performance concrete under the complex working condition are improved. The common silica fume of the iron alloy plant is applied and researched more as the admixture of the high-performance concrete, the mechanical property of the concrete is greatly improved, but the problems of source shortage, unstable performance, water requirement ratio in the concrete, drying shrinkage and the like also exist.
Because the bulk density of the silicon powder is small, the bulk density of the silicon powder is increased to about 0.5-0.6g/cm3 through a high densification measure for convenient transportation and storage in the industry, and the characteristic of large specific surface area of the silicon powder is damaged in the densification process. Meanwhile, the common silica powder has a large water ratio, so that the workability of concrete is poor, the defects of high dry shrinkage rate, easiness in cracking and the like of the concrete after the silica powder is added also affect the key factors of the application of the silica powder in the high-performance concrete, and restrict the large use of the silica powder.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention discloses a nano silicon-titanium powder material and a preparation method thereof.
The invention relates to a nano silicon-titanium powder material and a preparation method thereof, which comprises the following steps:
s1, uniformly mixing raw materials, and feeding the raw materials into a plasma electric furnace in a protective gas atmosphere; closing the furnace door, introducing hydrogen-containing protective gas into the furnace, heating, and carrying out high-temperature melt mixing; the melt mixing temperature is 2700-;
the raw material ratio is as follows: 30-60wt% of active silicon powder, 5-20wt% of gypsum powder, 3-15wt% of coarse titanium dioxide, 5-20wt% of high titanium slag tailings, 1-10wt% of bauxite,
the high titanium slag tailings are titanium slag containing more than 80 wt% of titanium oxide; the hydrogen-containing protective gas is a mixed gas of the protective gas and hydrogen, and the volume ratio of hydrogen is 15-18%;
s2, enabling the molten and mixed liquid flow to flow into a graphite cyclone separator, separating liquid silicon-containing raw materials, sending the liquid silicon-containing raw materials into a laser generator, directly radiating the molten raw materials by generated laser, and enabling the silicon-containing raw materials to quickly reach a boiling point and evaporate and gasify the silicon-containing raw materials into silicon vapor by utilizing a laser radiation effect;
silicon vapor above 2380 ℃ is sucked into a cooler and is rapidly cooled to 1120-1240 ℃, and the silicon vapor is mixed with other molten mixture and then is naturally cooled for subsequent treatment.
Preferably, the shielding gas is argon.
Preferably, the subsequent treatment specifically comprises: feeding into a crusher to be crushed into coarse blocks with the particle size of 50-100 mm; coarse blocks are subjected to coarse grinding and sieving to obtain coarse powder of 100-500 meshes; grinding aid is added into the coarse powder for ultra-fine treatment to obtain 3000-5000 meshes of micro powder;
and then the micro powder is subjected to interface treatment in the environment of 110-120 ℃, and simultaneously, a trace reinforcing agent is added for micro-compounding, and the micro powder is cooled and mixed by a cold mixer to output a finished product.
Preferably, the grinding aid is 3000-5000 mesh micropowder as described in step S2.
Preferably, the interface treatment is to add a coupling agent, and the addition volume ratio of the coupling agent to the micro powder is 0.5-2: 100.
A nano silicon-titanium powder material, which is prepared by any one of the methods.
By adopting the nano silicon-titanium powder material and the preparation method thereof, through introducing CaO, TiO2, Al2O3 and other components, the particle appearance is in a cornerite shape, is completely different from the shape of silicon ash and is in continuous gradation; the median diameter of the particles can reach 9-9.5um, and the specific surface area is 13000-15000m 2/kg; and further applied to concrete as an admixture, can improve the water demand ratio and the drying shrinkage problem of the concrete.
Drawings
FIG. 1 is a schematic view of a specific implementation flow of the method for preparing a nano-silicon-titanium powder material according to the present invention;
FIG. 2 is a photograph of the product obtained by the present invention.
Detailed Description
The following provides a more detailed description of the present invention.
The invention relates to a nano silicon-titanium powder material and a preparation method thereof, which comprises the following steps:
s1, uniformly mixing raw materials, and feeding the raw materials into a plasma electric furnace in a protective gas atmosphere; closing the furnace door, introducing hydrogen-containing protective gas into the furnace, heating, and carrying out high-temperature melt mixing; the melt mixing temperature is 2700-;
the raw material ratio is as follows: 30-60wt% of active silicon powder, 5-20wt% of gypsum powder, 3-15wt% of coarse titanium dioxide, 5-20wt% of high titanium slag tailings, 1-10wt% of bauxite,
the high titanium slag tailings are titanium slag containing more than 80 wt% of titanium oxide; the hydrogen-containing protective gas is a mixed gas of the protective gas and hydrogen, and the volume ratio of the hydrogen is 15-18%.
The oxidation can be avoided by using argon gas as protective gas, hydrogen-containing protective gas is introduced, and the hydrogen gas is ionized at high temperature, and then the number of titanium atom holes in the coarse titanium dioxide is increased by using the diffusion reduction effect and the hole reduction principle of hydrogen plasma, so that the surface activity of titanium is increased, and the titanium is not easy to polymerize and harden at high temperature.
S2, enabling the molten and mixed liquid flow to flow into a graphite cyclone separator, separating liquid silicon-containing raw materials, sending the liquid silicon-containing raw materials into a laser generator, directly radiating the molten raw materials by generated laser, and enabling the silicon-containing raw materials to quickly reach a boiling point and evaporate and gasify the silicon-containing raw materials into silicon vapor by utilizing a laser radiation effect;
silicon vapor above 2380 ℃ is sucked into a cooler and is rapidly cooled to 1120-1240 ℃, and the silicon vapor is mixed with other molten mixture and then is naturally cooled for subsequent treatment.
In the process, the liquid silicon-containing raw material is separated by utilizing the principle that various materials have different densities, silicon oxide is rapidly gasified under the action of laser, silicon steam is condensed in a high-temperature environment, and the long conical shape and the nano-micron high-quality silicon powder with high taper are formed in the cooling process under the action of gravity.
The plasma electric furnace is an electric furnace that heats or melts using plasma generated when a working gas is ionized. The apparatus for generating plasma, generally called plasma gun, includes two types, arc plasma gun and high frequency induction plasma gun. Working gas is introduced into a plasma gun, a device for generating an electric arc or a high-frequency (5-20 MHz) electric field is arranged in the gun, and the working gas is ionized after being acted to generate plasma consisting of electrons, positive ions, gas atoms and molecules. After the plasma is sprayed out from the nozzle of the plasma gun, high-speed and high-temperature plasma arc flame is formed, and the temperature is much higher than that of a common electric arc. The commonly used working gas is argon, which is a monatomic gas that is easily ionized, and an inert gas that protects the material. The working temperature can reach 20000 □, and the method is used for smelting special steel, titanium and titanium alloy, superconducting materials and the like.
Taking out the molten mixture, naturally cooling, and crushing into 50-100mm coarse blocks in a crusher; coarse blocks are coarsely ground into coarse powder of 100-500 meshes; grinding aid is added into the coarse powder for ultra-fining treatment to obtain 3000-6000-mesh micro powder; a small amount of 3000-mesh micropowder obtained by sieving coarse powder with a 3000-mesh sieve can be used as a grinding aid.
The micro powder is processed into intermediate material by interface treatment in the environment of 110-120 ℃, and simultaneously, the micro reinforcing agent is added for micro compounding, and the finished product is output after cooling and mixing by a cold mixer.
Using a coupling agent, adding 1-4 parts of the coupling agent per 100 parts by volume of the micro powder for interface treatment, and simultaneously adding 0.2-2 parts of a reinforcing agent.
Embodiment mode 1:
s1, uniformly mixing raw materials, and feeding the raw materials into a plasma electric furnace in a protective gas atmosphere; closing the furnace door, introducing hydrogen-containing protective gas into the furnace, heating, and carrying out high-temperature melt mixing; the melt mixing temperature is 2700-;
the raw material ratio is as follows: 50wt% of active silicon powder, 20wt% of gypsum powder, 15wt% of coarse titanium dioxide, 5wt% of high titanium slag tailings and 10wt% of bauxite,
the high titanium slag tailings are titanium slag containing more than 80 wt% of titanium oxide; the hydrogen-containing protective gas is a mixed gas of argon and hydrogen, and the volume ratio of hydrogen is 15%.
S2, enabling the molten and mixed liquid flow to flow into a graphite cyclone separator, separating liquid silicon-containing raw materials, sending the liquid silicon-containing raw materials into a laser generator, directly radiating the molten raw materials by generated laser, and enabling the silicon-containing raw materials to quickly reach a boiling point and evaporate and gasify the silicon-containing raw materials into silicon vapor by utilizing a laser radiation effect;
silicon vapor above 2380 ℃ is sucked into a cooler and is rapidly cooled to 1220-1240 ℃, and the silicon vapor is mixed with other melt and mixture and then is naturally cooled for subsequent treatment.
The subsequent processing is the same as in embodiment 2.
The control example was used: mixing cement, composite silicon powder, fly ash, sand, water and an additive according to the proportion of 32: 18:9: the concrete is prepared by mixing the components in a ratio of 21:19.8:0.2, and the concrete is tested by using a compensated concrete shrinkage tester according to the GB50119-2203 standard after the concrete is recovered to room temperature.
The products prepared in examples 2 and 3 were compared with the control product.
In both comparative examples, a plurality of samples were taken for comparison, and the shrinkage of example 2 was reduced by 5.8-9.7% compared to comparative example 1, wherein the shrinkage of silicon powder using specific example 2 was reduced by 6.0-9.7%, and the shrinkage of silicon powder using specific example 3 was reduced by 5.8-9.2%.
The foregoing is a description of preferred embodiments of the present invention, and the preferred embodiments in the preferred embodiments may be combined and combined in any combination, if not obviously contradictory or prerequisite to a certain preferred embodiment, and the specific parameters in the examples and the embodiments are only for the purpose of clearly illustrating the inventor's invention verification process and are not intended to limit the patent protection scope of the present invention, which is defined by the claims and the equivalent structural changes made by the content of the description of the present invention are also included in the protection scope of the present invention.
Claims (6)
1. A method for preparing a nano silicon-titanium powder material is characterized by comprising the following steps:
s1, uniformly mixing raw materials, and feeding the raw materials into a plasma electric furnace in a protective gas atmosphere; closing the furnace door, introducing hydrogen-containing protective gas into the furnace, heating, and carrying out high-temperature melt mixing; the melt mixing temperature is 2700-;
the raw material ratio is as follows: 30-60wt% of active silicon powder, 5-20wt% of gypsum powder, 3-15wt% of coarse titanium dioxide, 5-20wt% of high titanium slag tailings, 1-10wt% of bauxite,
the high titanium slag tailings are titanium slag containing more than 80 wt% of titanium oxide; the hydrogen-containing protective gas is a mixed gas of the protective gas and hydrogen, and the volume ratio of hydrogen is 15-18%;
s2, enabling the molten and mixed liquid flow to flow into a graphite cyclone separator, separating liquid silicon-containing raw materials, sending the liquid silicon-containing raw materials into a laser generator, directly radiating the molten raw materials by generated laser, and enabling the silicon-containing raw materials to quickly reach a boiling point and evaporate and gasify the silicon-containing raw materials into silicon vapor by utilizing a laser radiation effect;
silicon vapor above 2380 ℃ is sucked into a cooler and is rapidly cooled to 1120-1240 ℃, and the silicon vapor is mixed with other molten mixture and then is naturally cooled for subsequent treatment.
2. The method of claim 1, wherein the shielding gas is argon.
3. The method for preparing nano silicon-titanium powder material according to claim 1, wherein the subsequent treatment comprises: feeding into a crusher to be crushed into coarse blocks with the particle size of 50-100 mm; coarse blocks are subjected to coarse grinding and sieving to obtain coarse powder of 100-500 meshes; grinding aid is added into the coarse powder for ultra-fine treatment to obtain 3000-5000 meshes of micro powder;
and then the micro powder is subjected to interface treatment in the environment of 110-120 ℃, and simultaneously, a trace reinforcing agent is added for micro-compounding, and the micro powder is cooled and mixed by a cold mixer to output a finished product.
4. The method for preparing nano silicon-titanium powder material as claimed in claim 3, wherein the grinding aid is 3000-5000 mesh micropowder as described in step S2.
5. The method for preparing nano silicon-titanium powder material according to claim 3, wherein the interface treatment is adding a coupling agent, and the adding volume ratio of the coupling agent to the micro powder is 0.5-2: 100.
6. A nano-silicon-titanium powder material, characterized in that, it is prepared by the method of any one of claims 1 to 5.
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2021
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